ASTM D7771-13
(Test Method)Standard Test Method for Determination of Benzo-α-Pyrene (BaP) Content in Carbon Black
Standard Test Method for Determination of Benzo-α-Pyrene (BaP) Content in Carbon Black
SIGNIFICANCE AND USE
5.1 This test procedure is used to determine the concentration of BaP extracted from carbon black by the means of a Soxhlet extraction apparatus with toluene.
SCOPE
1.1 This test method covers the qualitative and quantitative determination of only benzo-α-pyrene (BaP), a specific polycyclic aromatic hydrocarbon (PAH), on carbon black. The procedure involves Soxhlet extraction with toluene and analysis by gas chromatography with mass spectrometry (GC/MS). This method is not intended to test for U.S. Food and Drug Administration (FDA 21 CFR 178.3297) compliance of carbon blacks used for indirect food contact applications.
1.2 Units—The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D7771 − 13
StandardTest Method for
Determination of Benzo-α-Pyrene (BaP) Content in Carbon
1
Black
This standard is issued under the fixed designation D7771; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2.3 Federal Standard:
21 CFR 178.3297 Indirect Food Additives: Adjuvants, Pro-
1.1 This test method covers the qualitative and quantitative
4
ductions Aids, and Sanitizers, Colorants for Polymers
determination of only benzo-α-pyrene (BaP), a specific poly-
cyclic aromatic hydrocarbon (PAH), on carbon black. The
3. Terminology
procedure involves Soxhlet extraction with toluene and analy-
3.1 Definitions of Terms Specific to This Standard:
sis by gas chromatography with mass spectrometry (GC/MS).
3.1.1 benzo-α-pyrene, BaP, n—also known as 3,4-
This method is not intended to test for U.S. Food and Drug
benzopyrene or benzo-a-pyrene is a specific polycyclic aro-
Administration (FDA21 CFR 178.3297) compliance of carbon
matic hydrocarbon (PAH) or polynuclear aromatic hydrocar-
blacks used for indirect food contact applications.
bon that consist of fused aromatic rings with no heteroatom or
1.2 Units—The values stated in SI units are to be regarded
substituent.
as the standard. No other units of measurement are included in
3.1.1.1 Discussion—PAHs naturally occur in oil, coal, and
this standard.
tar deposits; are produced by the incomplete combustion of
1.3 This standard does not purport to address all of the hydrocarbons;andoccurinmanyotherproductsandprocesses.
safety concerns, if any, associated with its use. It is the BaP is a pentacyclic PAH with the formula C H , related to
20 12
responsibility of the user of this standard to establish appro- pyrene by fusion of a phenylene group in the alpha position.
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use.
4.1 A portion of carbon black is Soxhlet extracted with
2. Referenced Documents
toluene for a specified period of time. The resultant extract is
2
purified by solid-phase extraction (SPE), concentrated down to
2.1 ASTM Standards:
a known volume, and subsequently analyzed for BaP by gas
D4483 Practice for Evaluating Precision for Test Method
chromatography with mass spectrometry (GC/MS). The BaP
Standards in the Rubber and Carbon Black Manufacturing
quantification is performed by the means of a deuterated
Industries
3
internal standard (isotope dilution).
2.2 EPA Standard:
Method 8270D Semivolatile Organic Compounds by Gas
5. Significance and Use
Chromatography/Mass Spectrometry (GC/MS)
5.1 This test procedure is used to determine the concentra-
tion of BaP extracted from carbon black by the means of a
1
This test method is under the jurisdiction ofASTM Committee D24 on Carbon
Soxhlet extraction apparatus with toluene.
Black and is the direct responsibility of Subcommittee D24.66 on Environment,
Health, and Safety.
6. Apparatus
Current edition approved Nov. 1, 2013. Published November 2013. Originally
approved in 2011. Last previous edition approved in 2011 as D7771 – 11. DOI: 6.1 Soxhlet Extractor with Reflux Condenser, 50- or 100-
3
10.1520/D7771-13.
cm capacity.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 6.2 Extraction Thimbles, glass or cellulose, approximately
3
Standards volume information, refer to the standard’s Document Summary page on
50- to 70-cm capacity. For instance, glass extraction thimble
the ASTM website.
3
Available from United States Environmental Protection Agency (EPA), Ariel
4
Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20004, http:// Available from the U.S. Government Printing Office, Superintendent of
www.epa.gov/epaoswer/hazwaste/test/new-meth.htm#8270D. Documents, 732 N. Capital St., NW., Washington, DC 20402-0001.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D7771 − 13
TABLE 1 Native and Deuterated BaP Compounds
of 35-mm diameter by 90-mm height with course porosity (70
to 100 µm similar to Ace Glass Size C, Porosity B, Code-14). PAH CAS# Deuterated PAH CAS#
Benzo(a)pyrene 50-32-8 d -Benzo(a)pyrene 63466-71-7
12
6.3 Heating Mantle,compatiblewithboilingflaskdescribed
in 6.4.
3
6.4 Boiling Flasks for Soxhlet, for example, 250 cm .
6.19 Manometer, capable of pressure readings in the range
of 5 6 0.3 kPa.
6.5 Glass Beads, approximately 180 to 250 µm (60/80
mesh) if glass thimbles are used. N
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D7771 − 11 D7771 − 13
Standard Test Method for
Determination of Benzo-α-Pyrene (BaP) Content in Carbon
1
Black
This standard is issued under the fixed designation D7771; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method covers the qualitative and quantitative determination of only benzo-α-pyrene (BaP), a specific polycyclic
aromatic hydrocarbon (PAH), on carbon black. The procedure involves Soxhlet extraction with toluene and analysis by gas
chromatography with mass spectrometry (GC/MS). This method is not intended to test for U.S. Food and Drug Administration
(FDA) (FDA 21 CFR 178.3297) compliance of carbon blacks used for indirect food contact applications.
1.2 Units—The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this
standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D4527D4483 Test Method for Carbon Black—Solvent ExtractablesPractice for Evaluating Precision for Test Method Standards
in the Rubber and Carbon Black Manufacturing Industries
3
2.2 EPA Standard:
Method 8270D Semivolatile Organic Compounds by Gas Chromatography/Mass Spectrometry (GC/MS)
2.3 Federal Standard:
4
21 CFR 178.3297 Indirect Food Additives: Adjuvants, Productions Aids, and Sanitizers, Colorants for Polymers
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 benzo-α-pyrene, BaP, n—also known as 3,4-benzopyrene or benzo-a-pyrene is a specific polycyclic aromatic hydrocarbon
(PAH) or polynuclear aromatic hydrocarbon that consist of fused aromatic rings with no heteroatom or substituent.
1
This test method is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.66 on Environment, Health,
and Safety.
Current edition approved Nov. 1, 2011Nov. 1, 2013. Published December 2011November 2013. Originally approved in 2011. Last previous edition approved in 2011 as
D7771 – 11. DOI: 10.1520/D7771-11.10.1520/D7771-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from United States Environmental Protection Agency (EPA), Ariel Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20004, http://www.epa.gov/
epaoswer/hazwaste/test/new-meth.htm#8270D.
4
Available from the U.S. Government Printing Office, Superintendent of Documents, 732 N. Capital St., NW., Washington, DC 20402-0001.
3.1.1.1 Discussion—
PAHs naturally occur in oil, coal, and tar deposits; are produced by the incomplete combustion of hydrocarbons; and occur in many
other products and processes. BaP is a pentacyclic PAH with the formula C H , related to pyrene by fusion of a phenylene group
20 12
in the alpha position.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D7771 − 13
4. Summary of Test Method
4.1 A portion of carbon black is Soxhlet extracted with toluene for a specified period of time. The resultant extract is purified
by solid-phase extraction (SPE), concentrated down to a known volume, and subsequently analyzed for BaP by gas
chromatography with mass spectrometry (GC/MS). The BaP quantification is performed by the means of a deuterated internal
standard (isotope dilution).
5. Significance and Use
5.1 This test procedure is used to determine the concentration of BaP extracted from carbon black by the means of a Soxhlet
extraction apparatus with toluene.
6. Apparatus
3
6.1 Soxhlet Extractor with Reflux Condenser, 50- or 100-cm capacity.
3
6.2 Extraction Thimbles, glass or cellulose, approximately 50- to 70-cm capacity. For instance, glass extraction thimble of
35-mm diameter by 90-mm height with course porosity (70 to 100 μm similar to Ace Glass Size C, Porosity B, Code-14).
6.3 Heating Mantle, c
...
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